Strategic deuteration of macromolecules can be used in combination with nuclear magnetic resonance (NMR), infrared analysis, and neutron-based probing methods, such as small angle neutron scattering (SANS), to obtain rich structural and dynamic information that may be inaccessible by other methods. Such methodology can be particularly important for molecules that do not crystallize, or where understanding of the solution structural and/or dynamic details is required. Acrylic-based macromolecules are ubiquitous in many materials used in daily life, and acrylic polymers with novel properties for new applications are highly sought. In many applications, it is both important yet challenging to elucidate the structure-function relationship for these macromolecules. Techniques such as neutron scattering can provide much insight into this relationship; however, the generally high cost of key monomers such as acrylic acid-d3 (D2C═CD-CO2H) has been an obstacle for researchers wishing to prepare strategically deuterated acrylic polymers. Although there exist a variety of examples for introducing the vinyl-d3 (2H3-acrylic) group as a substituent using D2CO and the Wittig reaction (e.g., P. Keller, et al., Macromolecules 35, pp. 581-584, 2002, and J. Pitlik, et al., J. Labelled Compd. Radiopharm. 39, pp. 999-1009, 1997), current methods for making deuterated acrylate salts and the corresponding acid, such as D2C═CD-CO2H or D2C═CD-CO2D, are generally complex, costly, and limited to small scale production.